PROCESSUS D'ENROBAGE DES CANAUX D'ECOULEMENT D'UN CONVERTISSEUR CATALYTIQUE EN NID D'ABEILLES AVEC ENROBAGE DE DISPERSION

PROCESS FOR THE COATING OF THE FLOW CHANNELS OF A HONEYCOMB CATALYTIC CONVERTER CARRIER WITH A DISPERSION COATING

Abrégé français

Un processus d'enrobage de canaux d'écoulement d'un support de catalyseur cylindrique en forme de nid d'abeilles avec enrobage de dispersion par le remplissage des canaux d'écoulement orientés verticalement avec une quantité de remplissage d'enrobage de dispersion par le biais de la surface inférieure du support de catalyseur et ultérieurement le vidage vers le bas et l'extraction de la clairance des canaux d'écoulement, ainsi que le séchage et la calcination du support de catalyseur, en passant par les étapes suivantes : a) remplissage des canaux d'écoulement avec une quantité de remplissage qui est environ 10 % supérieure au volume vide des canaux d'écoulement, de sorte que l'enrobage de dispersion passe sur la surface supérieure du support de catalyseur une fois le cycle de remplissage terminé, b) suppression de l'enrobage de dispersion en excès sur le dessus avant le vidage des canaux d'écoulement et c) vidage et extraction de la clairance des canaux d'écoulement par le biais d'une impulsion d'extraction, qui est générée en reliant un réservoir à vide avec la surface inférieure du support de catalyseur, auquel cas le temps entre le début du cycle de remplissage et la fin du vidage et l'extraction de la clairance ne dure pas plus de 5 secondes.

Abrégé anglais

A process for the coating of the flow channels of a cylindrical, honeycomb form catalyst carrier with a dispersion coating through filling of the vertically oriented flow channels with a fill quantity of the coating dispersion through the bottom face of the catalyst carrier and subsequent downward emptying and clearance extraction of the flow channels, as well as drying and calcination of the catalyst carrier, by the following steps: a) filling of the flow channels with a fill quantity that is about 10% greater than the empty volume of the flow channels, so that the coating dispersion goes over the upper face of the catalyst carrier after completion of the filling cycle, b) removal of the excess coating dispersion at the top before emptying of the flow channels and c) emptying and clearance extraction of the flow channels through an extraction impulse, which is generated by connection of a vacuum tank with the bottom face of the catalyst carrier, whereby the time between the beginning of the fill cycle and the end of the emptying and clearance extraction amounts to no more than 5 seconds.

Revendications

The embodiments of the invention in which an exclusive
property or privilege is claimed are defined as follows:
1. A process for coating a cylindrical, monolithic
honeycomb-form catalyst carrier with a coating dispersion,
said carrier having axially aligned flow channels arranged
in a grid over its cross sectional area, said carrier
having an upper and a bottom face, and said process
comprising the steps of:
a) bringing said carrier in an upright position so as to
orient the flow channels vertically;
b) filling said flow channels through the bottom face
with a volume of said coating dispersion which is about 10%
greater than the empty volume of the flow channels, so that
after completion of the filling cycle said upper face is
flooded by the coating dispersion;
c) removing excess coating dispersion from the upper face
of said carrier;
d) emptying and clearance extraction of the flow channels
through an extraction impulse, which is generated by
connecting a vacuum tank via an extraction conduit with the
bottom face of the catalyst carrier, whereby the time
between the beginning of the fill cycle and the end of the
emptying and clearance extraction amounts to no more than
about 5 seconds, and optionally drying and calcining the
24

coated catalyst carrier after said emptying and clearance
extraction of the flow channels.
2. The process according to claim 1, wherein said vacuum
tank has an initial partial vacuum of at least about 150
mbar and a volume which amounts to from about 100 to 1000
times the volume of the catalyst carrier.
3. The process according to claim 1 or 2, wherein during
said clearance extraction, a minimal air flow rate of about
m/s is maintained in the flow channels.
4. The process according to claim 1, 2 or 3, wherein said
extraction conduit has a cross sectional area and is
equipped with a throttle flap for allowing open flow of
said dispersion, the open flow cross sectional area of
which can be adjusted from between zero and the total cross
sectional area of the extraction conduit.
5. The process according to any one of claims 1 to 4,
wherein the time between the filling and the extraction
steps is short enough that the flow limit of the dispersion
cannot develop due to the thixotropic property or intrinsic
viscosity of said dispersion.
25

6. The process according to any one of claims 1 to 5,
wherein said catalyst carrier is moistened before coating.
7.The process according to any one of claims 1 to 5,
wherein said catalyst carrier is pre-impregnated with
acids, bases or saline solutions before coating.
8. The process according to any one of claims 1 to 7,
wherein after said emptying and clearance extraction of the
flow channels, and before calcining the catalyst carrier, a
heated flow of air with a temperature of between about 50
and 80° C. is conducted through the flow channels against
the emptying direction with a speed of more than about 2 to
20 m/s for a duration of from about 2 to 60 seconds.
9. A process for coating a honeycomb-form catalyst
carrier with a coating dispersion, said carrier having
axially aligned flow channels arranged in a grid over its
cross sectional area, said carrier having an upper and a
bottom face, and said process comprising the steps of:
a) bringing said carrier in an upright position so as to
orient the flow channels vertically;
b) filling said flow channels through the bottom face
with a volume of said coating dispersion which is greater
than the empty volume of the flow channels, so that after
36

completion of the filling cycle said upper face is covered
by the coating dispersion:
c) emptying and clearance extraction of the flow channels
through an extraction impulse, which is generated by
connecting a vacuum tank via an extraction conduit with the
bottom face of the catalyst carrier, whereby the time
between the beginning of the fill cycle and the end of the
emptying and clearance extraction amounts to no more than
about 5 seconds, and optionally drying and calcining the
coated catalyst carrier after said emptying and clearance
extraction of the flow channels.
27

Description

101520CA 02265071 1999-03-09PROCESS FOR THE COATING OF THE FLOW CHANNELS OF A HONEYCOMBFORM CATALYTIC CONVERTER CARRIER WITH A DISPERSION COATINGIntroduction and BackgroundThe present invention relates to a process for thecoating of the flow channels of a honeycomb form catalystcarrier with a dispersion coating.Catalytic converter carriers in honeycomb form are inlarge measure used for the creation of automobile exhaustcatalytic converters. They have a cylindrical shape, and arefilled with a multitude of flow channels parallel to the axisof the cylinder for the exhaust of internal combustion engines.The cross-sectional shape of the catalyst carrier depends onthe requirements of the vehicle design. In wide use arecatalytic converters with round, elliptical or triangularshaped cross-sections. The flow channels mostly have a squarecross-section and are arranged in a tight grid over the entirecross-section of the catalytic converter. According to theparticular application scenario, the cell density of the flowchannels varies between 10 and 120 cm“. Honeycomb carrierswith cell densities up to 250 cm” and more are being developed.Predominantly used for the purification of autoexhaust gas are catalyst carriers that are obtained throughextrusion of ceramic masses. Alternatively, catalyst carriersmade out of corrugated and wound up metal foils are available.101520CA 02265071 1999-03-09Ceramic catalyst carriers with cell densities of 62 cm“ arestill predominantly used today for the exhaust purification ofpassenger vehicles. The cross-sectional dimensions of the flowchannels in this case amount to 1.27 x 1.27 mm“. The wallthicknesses of these catalyst carriers lie between 0.1 and 0.2mm.For the most part, finely distributed platinum groupmetals, which can be changed in their catalytic effect throughcompounds of base metals, are used for the conversion ofpollutants contained in automobile exhaust - such as carbonmonoxide, hydrocarbons, and nitrogen oxide - into innocuouscompounds. These catalytically active components must bedeposited on the catalyst carriers. However, it is notpossible to guarantee the required fine distribution of thecatalytically active components through deposition of thesecomponents on the geometric surfaces of the catalyst carriers.This applies in the same way to non—porous metallic catalystcarriers as well as porous ceramic ones. A sufficiently largesurface area for the catalytically active components can onlybe made available through application of a support coating offine particulate, high surface area materials.Thus the present invention relates to a process forthe application of such a support coating on the inner surfacesof the flow channels of honeycomb form catalyst carriers.101520CA 02265071 1999-03-09Within the framework of this invention, the support coating forthe catalytically active components is designated as adispersion coating. The dispersion coating consists of fineparticulate high surface area materials and is produced underapplication of a so—called coating dispersion. The coatingdispersion for the most part involves a slurry of the fineparticulate materials in water.Various processes for the deposition of thedispersion coating on the catalyst carrier under application ofthe coating dispersion are known from the state of the art.After the coating process, the catalyst carriers are dried andthen calcined for the strengthening of the dispersion coating.Then the catalytically active components are introduced intothe dispersion coating through impregnation with mostly aqueoussolutions of precursor compounds of the catalytically activecomponents. Alternatively, the catalytically active componentscan be added to the coating dispersion itself. In this case,an additional impregnation of the prepared dispersion coatingwith the catalytically active components is no longernecessary.For effective purification of the exhaust gases ofinternal combustion engines, the volume of the catalystcarriers must have a sufficient dimension. Usually a ratio ofthe engine cylinder displacement to the volume of the catalyst101520CA 02265071 1999-03-09carrier of 1 : 2 to 2 : 1 is chosen. Thus catalyst carriertypical for automobiles have a volume of about 1 liter with adiameter of 100 mm (4 inches) and a length of 152 mm (6inches). The dry weight of the dispersion coating on suchcatalyst carriers is from 50 to 200 g/l volume of the catalystcarrier. With a cell density of 62 cm“, this corresponds to acalculated coating thickness of the dispersion coating of 20 to80 pm. Because of the capillary forces, the dispersion coatingas a rule is nevertheless very unevenly distributed over thecross section of the flow channels, with strong accumulationsof coating material in the corners of the channels andrelatively thin coating thicknesses on the centers of thechannel walls.Processes for the application of the dispersioncoating on the catalyst carriers must have a high productivitywith low amounts of rejects. They must therefore make itpossible to apply the entire quantity of coating on thecatalyst carrier in a single operational cycle. Multiplecoatings to attain the required coating thickness should beavoided. Moreover, the coating processes must assure that thecoating material does not clog the flow channels. Furthermore,it is generally required from such coating processes that theyavoid coating the outer covering of the catalyst carrier. Inso doing, expensive coating material and potentially expensive101520CA 02265071 1999-03-09catalytically active components can be saved.GB 1 515 733 describes a coating process for ceramiccatalyst carriers. The porous catalyst carriers are insertedupright, that is, with vertically oriented flow channels, in apressure tight coating tank and degassed through application ofa partial vacuum of 0.84 bar (25 inch mercury column). Nextthe coating dispersion is poured over the upper face of thecatalyst carrier into the coating tank and pressed into thepores of the catalyst carrier through application ofoverpressure. After withdrawal of the overpressure and openingof a release valve in the base of the coating tank, the excesscoating dispersion flows out of the flow channels of thecatalyst carrier. Finally, any channels blocked by coatingdispersion are blown open with compressed air blown from top tobottom. The cycle time of this coating process amounts to lessthan 1 % to 2 minutes.US 4,208,454 likewise describes a process for thecoating of porous ceramic catalyst carriers. The catalystcarriers to be coated are placed with their lower face on theopening of a collection tank in which the pressure is reducedby means of a high volume blower by 5 to 16 inches of watercolumn in relation to the atmospheric pressure. This partialvacuum is held constant during the entire coating time. Apredetermined volume of the coating dispersion is distributed101520CA 02265071 1999-03-09over the upper face of the catalyst carrier and steadily runthrough the flow channels into the collection tank. Thesuction cycle is maintained for about 30 seconds. After thefirst 5 seconds, the entire quantity of coating is run throughthe catalyst carrier. During the remaining time, the airflowing through the flow channels ensures that any flowchannels blocked by coating dispersion are opened. Thequantity of coating remaining on the catalyst carrier can beinfluenced by the duration of the overall suction time and bythe level of the partial vacuum. The axial uniformity of thecoating on the catalyst carrier can be improved by turning thecatalyst carrier after about half of the suction time and thensuctioning in the opposite direction. With this process,coating dispersions with 30 to 45 % solids content as well as aviscosity of from 60 to 3000 cps can be processed. Thepreferred solids content lies at 37 % by weight and thepreferred viscosity at 400 cps. The reproducibility of thequantity of coating is given at +/- 5 % in this process.EP 0157 651 likewise describes a process for thecoating of ceramic catalyst carriers with a predeterminedquantity of a coating dispersion. To accomplish this, the pre-weighed quantity of the coating dispersion is poured into anopen wide tank and the catalyst carrier with its bottom facedipped in the dispersion. Then the dispersion is sucked into101520CA 02265071 1999-03-09the flow channels through application of a light partialvacuum. In order to improve the axial uniformity of thecoating, it is recommended here also to have the coatingprocess proceed in two steps.In the first step, only about 50 to 85 % of theentire quantity of coating is poured into the tank and suckedinto the catalyst carrier. Afterwards, the catalyst carrier isturned and the remaining quantity of coating is suctioned inthe opposite direction. This coating process requires noseparate step for the opening of any closed flow channels. Thecycle time of this process amounts to less than 1 minute. Withthis process, coating dispersions that have a solids content ofbetween 35 and 52% and a viscosity of between 15 and 300 cpscan be processed.Us 5,182,140 describes a process for the coating ofceramic and metallic catalyst carriers. In this process, thecoating dispersion is pumped from underneath into thevertically placed catalyst carrier until the dispersion reachesa level completely above the upper face of the catalystcarrier. Then the coating dispersion is removed from thesubstrate through application of compressed air on the upperface of the catalyst carrier. In this way, any flow channelsthat are still closed are blown open. According to Example 1of this patent document, a level of the coating dispersion of 2101520CA 02265071 1999-03-09cm over the upper face of the catalyst carrier is used. Thecompressed air for the expulsion of the coating dispersion fromthe flow channels is introduced in two successive stages ofpressure. During the first 2 seconds after filling thecatalyst carrier, the coating dispersion is acted upon withcompressed air of 3.7 bar. This high pressure is sufficient toexpel the coating dispersion completely from the flow channelsduring the available 2 seconds. Afterwards, the compressed airpressure is reduced to 0.37 bar and the catalyst carrier actedupon twice with this pressure for 0.5 seconds each time. Withthis process, coating dispersions that have a specific densitybetween 1 and 2 g/ml and a viscosity of between 100 and 500 cpscan be processed.DE 40 40 150 C2 likewise describes a process for theeven coating of a honeycomb carrier made out of ceramic ormetal. For this process, the honeycomb carrier is submerged ina dipping barrel and filled with the coating dispersion frombelow. Afterwards, the honeycomb carrier is emptied againthrough blowing or suction. The honeycomb carrier is thenremoved from the dipping barrel and cleared with suction orblowing in a separate system in order to avoid blocked flowchannels. with this process, coating dispersions with solidscontent of between 48 and 64 % and viscosities from 50 to morethan 100 cps can be processed.101520CA 02265071 1999-03-09Exhaust catalytic converters for internal combustionengines are subject to continually increasing statutoryrequirements in relation to their conversion of pollutants andservice life. An increase of the service life of the catalyticconverters can be achieved through an improved catalyst recipeas well as through an increase of the amount of thecatalytically active components on the catalyst; However, ahigher quantity of catalytically active components alsorequires a higher loading of the catalyst carrier with coatingdispersion. ‘Improved conversion of pollutants can also beachieved through catalyst carriers with higher cell densities.In both cases — with the increase of the coating concentrationas well as with the increase of the cell density - the dangerin the coating process of clogging of the flow channels withcoating dispersion increases.It is therefore an object of the present invention tomake available a new coating process for ceramic and metalliccatalyst carriers in honeycomb form that distinguishes itselfby the following characteristics:- reproducible loading of the catalyst carrier of aproduction lot always with the same quantity of coatingdispersion— coating of the catalyst carrier with more than 200 g ofdry mass per liter of catalyst carrier volume101520CA 02265071 1999-03-09— coating of catalyst carriers with cell densities up to 250cm“— as uniform a radial and axial thickness of the coating aspossible- assured prevention of clogged flow channels~ as great an independence of the process from therheological characteristics of the coating dispersion aspossibleSummary of the InventionThe above and other objects are achieved inaccordance with the present invention by a process for thecoating of the flow channels of a cylindrically shaped,honeycomb form catalyst carrier with a dispersion coatingthrough filling of the vertically oriented flow channels with afill quantity of the coating dispersion through the bottom faceof the catalyst carrier and subsequent downward emptying andclearance extraction of the flow channels as well as drying andcalcination of the catalyst carrier. The process ischaracterized by the following steps:a) Filling of the flow channels with a fill quantity that isabout 10% greater than the empty volume of the flowchannels, so that the coating dispersion goes over theupper face of the catalyst carrier after completion of theCA 02265071 2003-08-18 Iam. » .mm NS11.Cmfiyflw ia-*:mn ..v CJ flu.” $12. n.,>.n.. . .. 7 . .\ ma)“  CA 02265071 2003-08-18 51..5. .:m 71Y1 VAcif,’ X L‘. I-If’ "'Exawingf33 gure 4Y5. mi aha ?rafieZnv&ntion l£&f&flC@ a.“N,/"..» «.,. .'= 1"»:24.4. avgab:d 101520CA 02265071 1999-03-09is assured that all flow channels of the catalyst carrier arefilled with coating dispersion. This is the case then, if therequired volume of the coating dispersion is about 10% greaterthan the empty volume of all flow channels of the honeycombcarrier together. Preferably, this excess coating dispersionis set at 1 to S % of the empty volume of the flow channels.This excess should, on the one hand, he kept as minimal aspossible, but, on the other hand, be sufficient to guaranteethe complete filling of all flow channels. Too great an excessof the coating dispersion leads to a flushing effect in theflow channels and with it to a reduction of the quantity ofcoating remaining on the catalyst carrier.The filling of the flow channels can occur in variousways. The possibility exists of pumping the coating dispersioninto the catalyst carrier from below, or, sucking it into thecatalyst carrier through application of a partial vacuum at itsupper face. Preferably, the coating dispersion is pumped in.The second measure — according to which the excesscoating dispersion is removed from the top before emptying andclearance extraction of the flow channels - of the processaccording to the invention also serves for the prevention ofthis flushing effect. This can happen, for example, through anapplication of suction at the top face of the catalyst carrierfrom the side or from above. A neglect of the removal of the101520CA 02265071 1999-03-09top excess coating dispersion before the emptying would have asa consequence that this top excess coating dispersion likewisehas to be extracted through the flow channels. The flushingeffect connected with this would reduce the quantity of coatingdeposited on the catalyst carrier.Tests have shown that through the prior removal ofthe excess coating dispersion, the quantity of coating that cancollect on the catalyst carrier can be increased by about 20 gdry mass per liter of catalytic converter volume.The rapid emptying and secure prevention of blockedflow channels is achieved through application of an extractionimpulse at the bottom face of the catalyst carrier. The shorttime of less than 1 second between filling and emptying leadsto the situation where the flow limit of thixotropic tointrinsically viscous dispersions cannot build up. Theextraction impulse is generated by means of a vacuum tank,which is connected with the bottom face of the catalystcarrier. Preferably, the vacuum tank is evacuated at a partialvacuum of at least 150 mbar. Through creation of theconnection between the bottom face of the catalyst carrier andthe vacuum tank, the coating dispersion is removed from theflow channels within a short time span of 1 to 1.5 seconds.The in-rushing air opens any flow channels that are stillblocked, which, within the context of this invention, is101520CA 02265071 1999-03-09characterized as clearance extraction, and leads to a reductionof the partial vacuum in the vacuum tank and thus to acontinuous decrease in the flow rate of the air in the flowchannels.The emptying characteristic can be influenced by 4parameters. Consequently, it involves the initial partialvacuum in the vacuum tank, the required power of the vacuumblower, the volume of the vacuum tank in relation to the volumeof the catalyst carrier and the open flow cross section betweenthe bottom face of the catalyst carrier and the vacuum tank.As rapid a removal of the coating dispersion from theflow channels as possible is achieved through a partial vacuumin the vacuum tank of at least 150 mbar. Afterwards, thepartial vacuum, as the driving force for the removal of thecoating dispersion from the flow channels and for thesubsequent air flow, should continually decrease in order toprevent to much coating material from being removed from theflow channels. This can happen through appropriatedimensioning of the volume of the vacuum tank and the blowerpower, and through adjustment - between 0 and a maximum valueequal to the chosen conduit cross-section between catalystcarrier and vacuum tank - by means of a reducing damper, of theopen flow cross-section between the catalyst carrier and thetank._ _101520CA 02265071 1999-03-09During the clearance extraction, the flow rate of theair in the flow channels is over 5 m/s. The maximum value ofthe flow rate at the beginning of the extraction is over 40m/s. These flow rates can be set through correspondingregulation of the reducing damper and the blower power.Dry ceramic catalyst carriers can produce aconsiderable suction capacity for the fluid phase of thecoating dispersion. In the coating of high cell densitycatalyst carriers with cell densities of 120 cm” and over, thisalready leads to a solidification of the coating dispersion,and in turn to a clogging of the flow channels during thefilling of the catalyst carriers. In order to be able also tocoat these catalyst carriers as per the described process, itis provided to moisten the catalyst carriers before thecoating. In this moistening, a pre—impregnation with acids,bases, or saline solutions can be used. The pre—impregnationfacilitates the formation of the coating on the channel wallsaccording to the sol-gel method. Through the contact of thecoating dispersion with the pre-impregnated channel walls, thepH value of the dispersion is shifted. In this way thedispersion is converted into a gel.The concentration of the coating dispersion on thecatalyst carrier can be increased in an another advantageousembodiment of the process according to the invention by flowing101520CA 02265071 1999-03-09preheated air through the catalyst carrier at temperaturesbetween 20 and ISUT and speeds of more than 4, preferably 7 -10 m/s, against gravitational force for the duration of 5 to 20seconds, after removal from the coating apparatus from below.Through this type of drying, before the actual calcination ofthe catalyst carriers, a tapering of the flow channels — or anarrowing of the channel on the bottom end of catalyst carriers- frequently observed with very high loading, can be avoided.This additional measure thus makes it possible to load thecatalyst carrier with a higher quantity of coating than usual,without the danger existing that the flow channels taper off,or narrow, during the drying and calcination cycle.The invention is now explained in greater detail withreference to some examples.According to Figure 1, the coating apparatus consistsof:- the catalyst carrier 1 to be coated,- a receptacle 17 for the catalyst carrier with a lower rubbercollar 2 and an upper rubber collar 2’,- an extraction funnel 3 underneath the receptacle for thecatalyst carrier,- an extraction conduit 4 that connects the extraction funnel3 to the vacuum tank 5 through the throttle flap 12,- a demister 6 in the vacuum tank as well as an vacuum blower101520CA 02265071 1999-03-097, which maintains a partial vacuum of about 150 to 500 mbarin the vacuum tank,— a recirculation conduit 8 as well as a pump 9 for therecirculation of the excess coating dispersion,- the tank 10 for the coating dispersion 19,- a pump 11 for pumping the coating dispersion into thecatalyst carrier,- a cover cap 13 with a relief valve 16 and suction line 15that enters into the extraction line 4, whereby the covercap can be swung up around pivot axis 14 and— a suction valve 18 in suction line 15.With this coating apparatus, the coating of a honeycombcarrier is carried out as follows:1. Close the throttle flap i2 and suction valve 18,2. Load the catalyst carrier 1 in the receptacle 2,3. Set the cover cap 13 on the upper rubber collar of thecatalyst carrier, opening the relief valve 16,4. Pump a fill quantity of the coating dispersion, whichis about 10% greater than the empty volume of the flowchannels (excess coating dispersion), into the catalystcarrier from below with the pump 11, V5. Open the suction valve 18 and suction off the topexcess coating dispersion from the upper face into thevacuum tank 5,101520CA 02265071 1999-03-096. Close the suction valve 18, open the cover and thenopen the throttle flap 12 to a pre-determined value forextracting the surplus coating dispersion in thecatalyst carrier (clearance extraction),7. Post extraction of air to open any flow channels thatstill might be clogged,8. Remove the catalyst carrier, and in some cases flowheated air through the catalyst carrier against theemptying direction in a separate apparatus.In the vacuum tank, the extracted coating dispersion iscollected and routed back into the storage tank 10 by means ofpump 9 through the return conduit 8.With the described apparatus, the following test series wereconducted:comparison Example 1:A series of 100 ceramic honeycomb carrier were providedwith a catalytic coating. All dispersionswere strongly thixotropic (definition of thixotropy accordingto DIN 13342).Data of the honeycomb carrierscell density 62 cm”CA 02265071 1999-03-09wall thickness 0.16 mmdiameter 101.6 mmlength 152.4 mmvolume 1.24 15 Data of the coating dispersionAlgy mixed oxide dispersionsolids contentviscosityProcess parameters10 fill timeexcess coating dispersionsuction time for excess dispersionVvncmxm conuiner/ Vhoncycombpartial vacuum p,15 throttle flap settingemptying time (extraction time)post extraction time(clearance extraction)60 % by weight400 mPa.s-1.5 s8 %no suction500350 mbar27g\0lsWith these coating parameters, a coating concentration of20 210 g dry mass per liter of catalyst carrier with a standarddeviation of a=8g was obtained.101520CA 02265071 1999-03-09Example 1The coating series of Comparison Example 1 was repeated.The excess quantity of coating dispersion was, however, suckedoff within 1 second this time before the emptying.The coating concentration achieved in this way amounted to235 g of dry mass per liter of catalyst carrier with a standarddeviation of a=5g.Example 2The coating series of Example 1 was repeated with asetting for the throttle flap of 25 % (25 % opening of themaximum flow cross section). The channels were still blockedafter the clearance extraction. Afterwards, a flow of airheated to 80T!was conducted through the flow channels of thecatalyst carrier from the bottom up at a rate of 5 m/s for theduration of 10 seconds. The channels opened and still remainedopen even after 10 minutes.The coating concentration thereby achieved amounted to 263g of dry mass per liter of catalyst carrier with a standarddeviation of a=6 g.Example 3A further series of 100 honeycomb carriers were coated asper Example 1. The honeycomb carriers were moistened before101520CA 02265071 1999-03-09the coating by dipping in ammonia water solution (pH = 8.5).All other parameters were identical with those of Example 1.The attained dry absorption of the honeycomb carriersamounted to 252 g/l with a standard deviation of 0 = 3 g.Examgl e 4A series of 100 high cell density ceramic honeycombcarriers were provided with a catalytic coating.Data of the honeycomb carrierscell density 120 cm“wall thickness 0.1 mmdiameter 152.2 mmlength 50.8 mmvolume .93 1Data of the coating dispersionA155 mixed oxide dispersionsolids content 50 % by weightviscosity 300 mPa.sProcess parametersfill time 1.0 sexcess coating dispersion S %101520CA 02265071 1999-03-09suction time for excessdispersion 1 sVvlcuum cont.Iiner/ Vhoncycomb 5 0 0partial vacuum p, 400 mbarthrottle flap setting 30 %emptying time (extraction time) 0.5 spost extraction time (clearanceextraction) 3 sWith these coating parameters, a coating concentration of315 g of dry mass per liter of catalyst carrier with a standarddeviation of a=10g was obtained.As the preceding examples show, through the measuresaccording to the invention, specifically removal of the topexcess coating dispersion before emptying of the honeycombcarriers and circulation of heated air through them against thedirection of emptying, the achievable coating concentrationscan be increased considerably. Thus, through removal of thetop excess coating dispersion, the increase of the coatingconcentration in Example 1 amounts to +12 % in relation toComparison Example 1. A further increase of the coatingconcentration of +12 % (+25 % in relation to Comparison Example1) was achieved through reduction of the open flow cross-section in clearance extraction of, and subsequent circulation_.22_.CA 02265071 2003-08-18aarriarfi,Thfi raprmfiufiibility mi the amating can be imgravaflccnfiifiarahiy through impraqmatiam of fiha homayaamb marrierfiwith fimmania wafiar swlufiimn.The graaant raaulta V&YQ wbtain&& with thg agyaratuw and?igure 3. ?ha praaaaw c&m, navartheieag, ha marriaé cut withno.éifzarantly Cmnfigurad agparatumea, am iamg an the fiagarihadprmmafiurai gtapfi ara fwilawefi.Further vaxiatimna and mndificatimns Q? tha fsraqmimq willha aggarant ta thage fikiiiad in tha art anfi ar& ifltanfiad ta %amnmmmpaaaafi by flha ciaimfi appamdafi heretwg

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